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Hydroxyamine hydrochloride → (NE)-N-[(4-bromo-2,5-difluorophenyl)methylidene]hydroxylamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 反応物 | 4-Bromo-2,5-difluorobenzaldehyde | HCID 22489081 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 溶媒 | Ammonium Chloride | HCID 25517 | — |
| 生成物 | (NE)-N-[(4-bromo-2,5-difluorophenyl)methylidene]hydroxylamine | HCID 90310471 | 53.5% |
反応手順
A solution of 4-bromo-2,5-difluorobenzaldehyde (7.0 g, 31.67 mmol), hydroxyl amine hydrochloride (2.42 g, 34.84 mmol) in pyridine (35 mL) and ethanol (35 mL) was stirred at room temperature for 30 min. The reaction mixture was diluted with saturated ammonium chloride solution and extracted with ethyl acetate. The organic phase was washed with saturated brine solution, dried (Na2SO4), filtered, and concentrated under reduced pressure. The crude product was purified by flash chromatography (SiO2, eluting with 5-100% ethyl acetate in hexanes) to provide the title compound as a yellow solid (4.0 g, 53%): ESIMS m/z 238 [(M+2H)+].
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09113629B2 |
| 出典データセット | uspto-grants-2015_08 |
| ORD ID | ord-2b742c3ec23b4560b2f4e16afbf75d16 |
| 出典メモ | uspto-grants-2015_08 |